One-pot hydrothermal synthesis of FeNbO4 microspheres for effective sonocatalysis.

FeNbO4 sonocatalysts were successfully synthesized by a simple hydrothermal route at pH values of 3, 5, 7, 9 and 11. The catalysts were characterized by XRD, XPS, TEM, SEM, N2 adsorption and DRS to analyse the effect of pH parameters on the physicochemical properties of the materials during hydrothermal synthesis. The sonocatalytic activity of FeNbO4 microspheres was evaluated by using acid orange 7 (AO7) as the simulated contaminant. The experimental results showed that the best sonocatalytic degradation ratio (97.45%) of organic dyes could be obtained under the conditions of an initial AO7 concentration of 10 mg L-1, an ultrasonic power of 200 W, a catalyst dosage of 1.0 g L-1, and a pH of 3. Moreover, the sonocatalysts demonstrated consistent durability and stability across multiple test cycles. After active species capture experiments and calculation of the energy band, a possible mechanism was proposed based on the special Fenton-like mechanism and the dissociation of H2O2. This research shows that FeNbO4 microspheres can be used as sonocatalysts for the purification of organic wastewater, which has a promising application prospect.

Shape-Controlled Synthesis of Cu3TeO6 Nanoparticles with Photocatalytic Features.

Cu3TeO6 (CTO) has been synthesized by hydrothermal synthesis applying different pH values without any template or a calcination step to control the crystalline phase and the morphology of nanoparticles. The physicochemical properties characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, N2 adsorption, X-ray photoelectron spectroscopy, and diffuse reflectance ultraviolet-visible (DRUV-vis) spectroscopy techniques revealed that the pH values significantly influence the crystal growth. In acidic media (pH = 2), crystal growth has not been achieved. At pH = 4, the yield is low (10%), and the CTO presents irregular morphology. At pH = 6, the yield increases (up to 71%) obtaining an agglomeration of nanoparticles into spherical morphology. At basic conditions (pH = 8), the yield increases up to 90% and the morphology is the same as the sample obtained at pH = 6. At high basic conditions (pH = 10), the yield is similar (92%), although the morphology changes totally to dispersed nanoparticles. Importantly, the as-prepared CTO semiconductor presents photocatalytic activity for H2 production using triethanolamine as a sacrificial agent under visible light illumination. The results also revealed that the nanoparticles agglomerated in a spherical morphology with larger surface area presented almost double activities in H2 production compared to heterogeneously sized particles. These results highlight the suitable optoelectronic properties, including optical band gap, energy levels, and photoconductivity of CTO semiconductors for their use in photocatalytic H2 production.

Hydrothermal Synthesis of Ni3TeO6 and Cu3TeO6 Nanostructures for Magnetic and Photoconductivity Applications.

Despite great attention toward transition metal tellurates especially M3TeO6 (M = transition metal) in magnetoelectric applications, control on single phasic morphology-oriented growth of these tellurates at the nanoscale is still missing. Herein, a hydrothermal synthesis is performed to synthesize single-phased nanocrystals of two metal tellurates, i.e., Ni3TeO6 (NTO with average particle size ∼37 nm) and Cu3TeO6 (CTO ∼ 140 nm), using NaOH as an additive. This method favors the synthesis of pure NTO and CTO nanoparticles without the incorporation of Na at pH = 7 in MTO crystal structures such as Na2M2TeO6, as it happens in conventional synthesis approaches such as solid-state reaction and/or coprecipitation. Systematic characterization techniques utilizing in-house and synchrotron-based characterization methods for the morphological, structural, electronic, magnetic, and photoconductivity properties of nanomaterials showed the absence of Na in individual particulate single-phase MTO nanocrystals. Prepared MTO nanocrystals also exhibit slightly higher antiferromagnetic interactions (e.g., T N-NTO = 57 K and T N-CTO = 68 K) compared to previously reported MTO single crystals. Interestingly, NTO and CTO show not only a semiconducting nature but also photoconductivity. The proposed design scheme opens the door to any metal tellurates for controllable synthesis toward different applications. Moreover, the photoconductivity results of MTO nanomaterials prepared serve as a preliminary proof of concept for potential application as photodetectors.

Theoretical prediction and shape-controlled synthesis of two-dimensional semiconductive Ni3TeO6.

Current progress in two-dimensional (2D) materials explorations leads to constant specie enrichments of possible advanced materials down to two dimensions. The metal chalcogenide-based 2D materials are promising grounds where many adjacent territories are waiting to be explored. Here, a stable monolayer Ni3TeO6 (NTO) structure was computationally predicted and its stacked 2D nanosheets experimentally synthesized. Theoretical design undergoes featuring coordination of metalloid chalcogen, slicing the bulk structure, geometrical optimizations and stability study. The predicted layered NTO structure is realized in nanometer-thick nanosheets via a one-pot shape-controlled hydrothermal synthesis. Compared to the bulk, the 2D NTO own a lowered bandgap energy, more sensitive wavelength selectivity and an emerging photocatalytic hydrogen evolution ability under visible light. Beside a new 2D NTO with the optoelectrical and photocatalytic merits, its existing polar space group, structural specification, and design route are hoped to benefit 2D semiconductor innovations both in species enrichment and future applications.

Synthesis of TiO2/Nanozeolite Composites for Highly Efficient Photocatalytic Oxidation of Propene in the Gas Phase.

In this work, we reported the preparation of composites based on titania (TiO2) and Zeolite Socony Mobil-5 (ZSM-5) nanozeolite, following two approaches (i.e., incorporating the presynthesized zeolite in the synthesis medium of TiO2 and incorporating presynthesized TiO2 in the synthesis medium of ZSM-5). The materials synthesized were characterized by X-ray fluorescence (XRF), X-ray diffraction (XRD), nitrogen adsorption, X-ray photoelectron spectroscopy (XPS), ultraviolet-visible spectroscopy (UV-vis), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray (EDX) spectrometry analysis, and their photocatalytic activities were assessed in the oxidation of propene in the gas phase. It was observed that the synthesis methodology affects the final properties of the composite, which ultimately affected their photocatalytic performance in the studied application. It was found that the Nano-ZSM5/TiO2 composite was the most active among the investigated samples, which was attributed to the intimate contact between the two components of the composite, the preserved properties of the photocatalytic active phase in the final material, and the positive contribution of the nanozeolite by increasing the local concentration of propene.

Photocatalytic Oxidation of VOCs in Gas Phase Using Capillary Microreactors with Commercial TiO2 (P25) Fillings.

The elimination of volatile organic compounds (VOCs) at low concentration is a subject of great interest because these compounds are very harmful for the environment and human health. In this work, we have developed an easy methodology to immobilize a benchmark photocatalyst (P25) inside a capillary microreactor (Fused silica capillary with UV transparent coating) without any previous treatment. For this purpose, a dispersion of the sample (P25) in EtOH was used obtaining a packed bed configuration. We have improved the immobilization of the benchmark photocatalyst (P25) inside the capillary incorporating a surfactant (F-127) to generate porosity inside the microreactor to avoid severe pressure drops (∆P < 0.5 bar). The resulting capillaries were characterized by Scanning Electron Microscopy (SEM). These microreactors show a good performance in the abatement of propene (VOC) under flow conditions per mol of active phase (P25) due to an improved mass transfer when the photocatalyst is inside the capillary. Moreover, the prepared microreactors present a higher CO2 production rate (mole CO2/(mole P25·s)) with respect to the same TiO2 operating in a conventional reactor. The microreactor with low pressure drop is very interesting for the abatement of the VOCs since it improves the photoactivity of P25 per mol of TiO2 operating at near atmospheric pressure.

Synthesis of TiO2 with Hierarchical Porosity for the Photooxidation of Propene.

The elimination of volatile organic compounds (VOCs) at low concentration is a subject of great interest because these compounds are very harmful for the environment and human health. In this work, we have developed a synthesis methodology of TiO2 that allows obtaining meso-macroporous materials with hierarchical porosity and with high thermal stability for their application as photocatalysts in the removal of VOCs, specifically propene. The materials synthesized in this work were characterized by Scanning electron microscope (SEM), Transmission electron microscopy (TEM), powder X-ray diffraction (XRD), Thermogravimetric Analysis (TG), and nitrogen adsorption. It is observed that the samples calcined at 250 °C and 500 °C present a high photoactivity for the photooxidation of propene, which is similar to the benchmark material P25 (commercial TiO2). Moreover, the textural properties are better than those for P25, indicating that the samples are interesting for the preparation of photocatalysts with different conformations, such as in the form of coatings and fillings in different size scales.